A kind of synthetic method of 1-(2-pyridyl)-pyrazole-3-carboxylic acid and its derivatives
A technology of pyrazole dicarboxylic acid and derivatives, which is applied in organic chemistry methods, organic chemistry and other directions, can solve the problems of complicated synthesis process, high material cost, low final yield and the like, and achieves simple synthesis steps, low production cost, and improved The effect of efficiency
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Embodiment 1
[0075] Example 1 Preparation of 1-(2-pyridyl)-pyrazole-3-carboxylic acid and derivatives thereof
[0076] Step 1: Add 174.0mg 3,5-pyrazoledicarboxylic acid monohydrate and 250.0mg copper sulfate pentahydrate powder to a 25mL reactor, add 5mL pyridine and 10mL water, stir for 15 minutes, then put the reactor into an oven heated to 180°C in medium temperature, and reacted for 24 hours;
[0077] Step 2: After the reaction is over, transfer the reaction solution to a flask, add 2 mL of saturated sodium sulfide aqueous solution to the reaction solution, and filter after the precipitation is complete;
[0078] The third step: add 1M hydrochloric acid solution dropwise to the filtrate obtained in the second step, adjust the pH of the solution to 3, and filter;
[0079] The fourth step: use the organic solvent dichloromethane to extract the filtrate obtained in the third step (3×20 mL), collect the organic phase, and dry it with anhydrous sodium sulfate for 10 h;
[0080] The fifth ...
Embodiment 2
[0081] Example 2 Preparation of 1-(2-pyridyl)-pyrazole-3-carboxylic acid and derivatives thereof
[0082] Step 1: Add 174.0mg 3,5-pyrazoledicarboxylic acid monohydrate and 250.0mg copper sulfate pentahydrate powder to a 25mL reactor, add 5mL 3-methylpyridine and 10mL water, stir for 15 minutes, and then react The kettle was put into an oven and heated to 180°C, and reacted for 24 hours;
[0083] Step 2: After the reaction is over, transfer the reaction solution to a flask, add 2 mL of saturated sodium sulfide aqueous solution to the reaction solution, and filter after the precipitation is complete;
[0084] The third step: add 1M hydrochloric acid solution dropwise to the filtrate obtained in the second step, adjust the pH of the solution to 3, and filter;
[0085] The fourth step: use the organic solvent dichloromethane to extract the filtrate obtained in the third step (3×20 mL), collect the organic phase, and dry it with anhydrous sodium sulfate for 10 h;
[0086] The fif...
Embodiment 3
[0087] Example 3 Preparation of 1-(2-pyridyl)-pyrazole-3-carboxylic acid and its derivatives
[0088] Step 1: Add 174.0mg 3,5-pyrazoledicarboxylic acid monohydrate and 250.0mg copper sulfate pentahydrate powder to a 25mL reactor, add 5mL 4-picoline and 10mL water, stir for 15 minutes, and then react The kettle was put into an oven and heated to 180°C, and reacted for 24 hours;
[0089] Step 2: After the reaction is over, transfer the reaction solution to a flask, add 2 mL of saturated sodium sulfide aqueous solution to the reaction solution, and filter after the precipitation is complete;
[0090] The third step: add 1M hydrochloric acid solution dropwise to the filtrate obtained in the second step, adjust the pH of the solution to 3, and filter;
[0091] The fourth step: use the organic solvent dichloromethane to extract the filtrate obtained in the third step (3×20 mL), collect the organic phase, and dry it with anhydrous sodium sulfate for 10 h;
[0092] The fifth step: C...
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